HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 178482927, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,4-Dichloro-5-fluoropyrimidine | HCID 250705 | — |
| Reactant | HCID 178482959 | HCID 178482959 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 178482927 | HCID 178482927 | 39% |
Reaction Steps
2,4-dichloro-5-fluoropyrimidine (166 mg, 1 mmol), N5,N5-dimethyl-1H-pyrazole-3,5-diamine (Method 34, 150 mg, 1.2 mmol), and DIEA (0.35 ml, 2 mmol) in ethanol (3 ml) was heated at 55° C. overnight. Solvent was removed, and the residue was purified by silica gel chromatography (by ISCO Combiflash with a gradient of 0-5% methanol in methylene chloride with 1% NH4OH). 100 mg product was obtained as a white solid (40%). MS: 257 (M+1); NMR (DMSO-d6, 400 MHz, 80° C.) δ11.60 (br, 1H), 10.26 (br, 1H), 8.23 (s, 1H), 5.73 (s, 1H), 2.76 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08088784B2 |
| Source dataset | uspto-grants-2012_01 |
| ORD ID | ord-4e47db7c8a5946159acb41d43c4e18e5 |
| Source note | uspto-grants-2012_01 |